KR102349084B1 - Method of manufacturing a aramid non-woven fabric with copolymerized aramid film - Google Patents
Method of manufacturing a aramid non-woven fabric with copolymerized aramid film Download PDFInfo
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- KR102349084B1 KR102349084B1 KR1020160048676A KR20160048676A KR102349084B1 KR 102349084 B1 KR102349084 B1 KR 102349084B1 KR 1020160048676 A KR1020160048676 A KR 1020160048676A KR 20160048676 A KR20160048676 A KR 20160048676A KR 102349084 B1 KR102349084 B1 KR 102349084B1
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- nonwoven fabric
- aromatic group
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/4334—Polyamides
- D04H1/4342—Aromatic polyamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
- D04H1/498—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres entanglement of layered webs
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
- D10B2331/021—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides aromatic polyamides, e.g. aramides
Abstract
본 발명은 공중합 아라미드 필름을 이용한 아라미드 부직포의 제조방법에 관한 것으로서, (ⅰ) 유기용매에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액을 필름상으로 캐스팅하여 제조된 공중합 아라미드 필름을 리본 형태로 슬리팅(Slitting)하는 공정; 및 (ⅱ) 리본 형태로 슬리팅된 공중합 아라미드 필름을 적층한 후 니들펀칭하는 공정;을 포함한다.
본 발명은 일정농도에서 액정성을 발현하는 공중합 아라미드 중합용액으로 제조되어 일축방향으로만 배향된 공중합 아라미드 필름을 사용하여 아라미드 부직포를 제조하기 때문에, 상기 니들펀칭공정에서 적층된 리본 형태의 공중합 아라미드 필름이 일측방향으로 쉽게 갈라지거나 찢어져 부직포를 형성할 수 있게 된다. 그로인해 본 발명은 종래 아라미드 부직포 제조를 위해 공중합 아라미드 중합용액을 섬유상으로 방사하는 공정을 생략할 수 있어서 제조공정이 간소화 된다.The present invention relates to a method for manufacturing an aramid nonwoven fabric using a copolymerized aramid film, (i) casting a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent into a film slitting the prepared copolymer aramid film in the form of a ribbon; and (ii) a step of needle punching after laminating the copolymer aramid film slitted in the form of a ribbon.
The present invention is prepared with a copolymer aramid polymerization solution that expresses liquid crystallinity at a certain concentration and uses a copolymer aramid film oriented only in uniaxial direction to prepare an aramid nonwoven fabric, so the copolymer aramid film in the form of a ribbon laminated in the needle punching process It is easily cracked or torn in one direction to form a nonwoven fabric. Therefore, the present invention can omit the process of spinning the copolymerized aramid polymerization solution into fibers for the production of the conventional aramid nonwoven fabric, thereby simplifying the manufacturing process.
Description
본 발명은 공중합 아라미드 필름을 이용한 아라미드 부직포의 제조방법에 관한 것으로서, 구체적으로는 아라미드 섬유의 방사공정 없이도 아라미드 부직포를 제조할 수 있는 방법에 관한 것이다.The present invention relates to a method for manufacturing an aramid nonwoven fabric using a copolymerized aramid film, and more particularly, to a method capable of manufacturing an aramid nonwoven fabric without a spinning process of aramid fibers.
아라미드 부직포를 제조하는 종래방법으로는 아라미드 중합체를 황산에 용해시켜 제조한 방사용액(방사도프)를 방사구금을 통해 방사하여 아라미드 필라멘트(장섬유)를 제조한 다음, 이를 일정길이로 절단하여 아라미드 스테이플(단섬유)를 제조한 다음, 아라미드 단섬유를 웹(Web) 상태로 적층한 후 니들펀칭하는 방법이 널리 사용되어 왔다.In a conventional method for manufacturing an aramid nonwoven fabric, an aramid filament (long fiber) is prepared by spinning a spinning solution (spun dope) prepared by dissolving an aramid polymer in sulfuric acid through a spinneret, and then cutting it to a certain length to obtain aramid staples. After manufacturing (short fibers), and then laminating the short aramid fibers in a web state, a method of needle punching has been widely used.
아라미드 부직포를 제조하는 또 다른 종래기술로는 아라미드 중합체를 황산에 용해시켜 제조한 방사용액(방사도프)를 방사구금을 통해 방사하여 아라미드 필라멘트(장섬유)를 제조하는 방사공정 중에 방사되는 아라미드 필라멘트(장섬유)들을 서로 교락시켜 스펀본드(Spunbond) 타입인 아라미드 부직포를 제조하는 방법도 사용되어 왔다.As another prior art for manufacturing aramid nonwoven fabric, a spinning solution (spun dope) prepared by dissolving an aramid polymer in sulfuric acid is spun through a spinneret to produce aramid filaments (long fibers). Long fibers) have been entangled with each other to produce a spunbond-type aramid nonwoven fabric.
그러나, 상기의 종래방법들은 아라미드 필라멘트를 제조하는 방사공정을 거처야하기 때문에 방사장치 및 제조공정이 복잡해지는 문제가 있었고, 아울러 상기 방사용액 내에 황산이 포함되어 있어서 방사장치가 심하게 부식되는 문제가 있었다.However, the above conventional methods have a problem in that the spinning device and the manufacturing process are complicated because it has to go through a spinning process to produce an aramid filament, and also there is a problem in that the spinning device is severely corroded because sulfuric acid is contained in the spinning solution. .
본 발명의 과제는 공중합 아라미드 필름을 이용하여 아라미드 필라멘트(장섬유)를 제조하기 위한 방사공정 없이도 아라미드 부직포를 제조할 수 있는 방법을 제공하는 것이다.An object of the present invention is to provide a method capable of producing an aramid nonwoven fabric without a spinning process for producing an aramid filament (long fiber) using a copolymerized aramid film.
이와같은 과제를 달성하기 위해서, 본 발명에서는 (ⅰ) 유기용매에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합 중합체가 용해되어 있는 중합용액을 필름상으로 캐스팅하여 공중합 아라미드 필름을 제조한 다음, (ⅱ) 상기 공중합 아라미드 필름을 리본 형태로 슬리팅(Slitting)하고, (ⅲ) 리본 형태로 슬리팅된 공중합 아라미드 필름을 적층한 후 니들펀칭하여 아라미드 부직포를 제조한다.In order to achieve the above object, in the present invention, (i) a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent is cast into a film to prepare a copolymer aramid film Then, (ii) slitting the copolymer aramid film in the form of a ribbon, (iii) laminating the copolymer aramid film slitted in the form of a ribbon, and then needle punching to prepare an aramid nonwoven fabric.
본 발명은 일정농도에서 액정성을 발현하는 공중합 아라미드 중합용액으로 제조되어 일축방향으로만 배향된 공중합 아라미드 필름을 사용하여 아라미드 부직포를 제조하기 때문에, 상기 니들펀칭공정에서 적층된 리본 형태의 공중합 아라미드 필름이 일측방향으로 쉽게 갈라지거나 찢어져 부직포를 형성할 수 있게 된다. 그로인해 본 발명은 종래 아라미드 부직포 제조를 위해 공중합 아라미드 중합용액을 필라멘트(장섬유)로 방사하는 공정을 생략할 수 있어서 제조공정이 간소화 된다.The present invention is prepared with a copolymer aramid polymerization solution that expresses liquid crystallinity at a certain concentration and uses a copolymer aramid film oriented only in uniaxial direction to prepare an aramid nonwoven fabric, so the copolymer aramid film in the form of a ribbon laminated in the needle punching process It is easily cracked or torn in one direction to form a nonwoven fabric. Therefore, the present invention can omit the process of spinning the copolymerized aramid polymerization solution into a filament (long fiber) for the production of a conventional aramid nonwoven fabric, thereby simplifying the manufacturing process.
이하, 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.
본 발명에 따른 공중합 아라미드 필름을 이용한 아라미드 부직포의 제조방법은 (ⅰ) 유기용매에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액을 필름상으로 캐스팅하여 제조된 공중합 아라미드 필름을 리본 형태로 슬리팅(Slitting)하는 공정; 및 (ⅱ) 리본 형태로 슬리팅된 공중합 아라미드 필름을 적층한 후 니들펀칭하는 공정;을 포함한다.The method for producing an aramid nonwoven fabric using a copolymerized aramid film according to the present invention is (i) a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent in the form of a film by casting slitting the copolymerized aramid film in the form of a ribbon; and (ii) a step of needle punching after laminating the copolymer aramid film slitted in the form of a ribbon.
상기 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체는 하기 일반식(Ⅰ)의 반복단위를 갖는다.The aramid copolymer including an aromatic group substituted with the cyano group (-CN) has a repeating unit of the following general formula (I).
[상기 식(Ⅰ)에서 Ar은 하기 일반식(Ⅱ)의 방향족기고, 상기 A는 하기 일반식(Ⅲ)의 방향족기 이거나 하기 일반식(Ⅱ)의 방향족기와 일반식(Ⅲ)의 방향족기의 비율이 1:9~9:1인 방향족기 이다][In the formula (I), Ar is an aromatic group of the following general formula (II), and A is an aromatic group of the following general formula (III) or an aromatic group of the following general formula (II) It is an aromatic group with a ratio of 1:9 to 9:1]
구체적으로, 본 발명은 먼저 유기용매에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액을 T-다이(T-Die) 또는 닥터블레이드 등을 이용하여 필름형태로 캐스팅하여 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체로 이루어진 공중합 아라미드 필름을 제조한다.Specifically, the present invention is a film form using a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent first using a T-die or a doctor blade. Casting to prepare a copolymerized aramid film made of an aramid copolymer containing an aromatic group substituted with a cyano group (-CN).
상기 공중합 아라미드 필름을 제조하는 구현일례로서, 상기 중합용액을 T-다이(T-Die)를 통해 벨트 또는 유리판 상에 캐스팅한 후, 차례로 응고/수세/열처리하여 공중합 아라미드 필름을 제조할 수도 있고, 상기 중합용액을 닥터블레이드를 이용하여 유리판 상에 캐스팅한 후, 응고/수세/열처리하여 공중합 아라미드 필름을 제조할 수 있다.As an embodiment of manufacturing the copolymer aramid film, the polymerization solution is cast on a belt or a glass plate through a T-die, and then coagulated / washed / heat-treated to prepare a copolymer aramid film, After casting the polymerization solution on a glass plate using a doctor blade, it is possible to prepare a copolymerized aramid film by coagulation/washing/heat treatment.
본 발명에서는 상기 공중합 아라미드 필름을 제조하는 방법을 특별하게 한정하지 않는다.In the present invention, the method for producing the copolymer aramid film is not particularly limited.
상기 공중합 아라미드 필름의 두께는 10~50 ㎛인 것이 바람직하다.The thickness of the copolymer aramid film is preferably 10 to 50 ㎛.
이때, 유기용매에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 상기 중합용매는 구현일례로서 무기염이 첨가된 유기용매에 방향족 디아민 성분으로 파라페닐렌디아민과 시아노-파라-페닐렌 디아민을 1:9 ~ 9:1의 몰비로 용해시키거나 시아노-파라-페닐렌 디아민을 단독으로 용해시킨 다음, 상기 유기용매에 테레프탈로일 디클로라이드를 상기 방향족 디아민 성분의 총량과 동일한 몰량(Molar account)으로 첨가, 반응시켜 제조한다.In this case, the polymerization solvent in which an aramid copolymer including an aromatic group substituted with a cyano group (-CN) is dissolved in the organic solvent is an embodiment, as an example, paraphenylenediamine and cyano No-para-phenylene diamine is dissolved in a molar ratio of 1:9 to 9:1 or cyano-para-phenylene diamine is dissolved alone, and then terephthaloyl dichloride is added to the aromatic diamine component in the organic solvent. It is prepared by adding and reacting in the same molar amount as the total amount of
상기 유기용매는 N-메틸-2-피롤리돈, N,N-디메틸아세트아미드, 헥사메틸포스포아미드, N,N,N',N'-테트라메틸우레아 또는 N,N-디메틸포름아미드 등이다.The organic solvent is N-methyl-2-pyrrolidone, N,N-dimethylacetamide, hexamethylphosphoamide, N,N,N',N'-tetramethylurea or N,N-dimethylformamide, etc. to be.
다음으로, 본 발명은 상기와 같이 제조된 일반식(Ⅰ)의 공중합 아라미드 필름을 폭이 10㎜ 정도인 리본 형태로 슬리팅(Slitting)한 후, 리본 형태로 슬리팅된 공중합 아라미드 필름을 적층한 후, 니들펀칭을 실시하여 아라미드 부직포를 제조한다.Next, the present invention slitting the copolymer aramid film of the general formula (I) prepared as above in a ribbon form having a width of about 10 mm (Slitting), and then laminating the copolymer aramid film slit in the form of a ribbon After that, needle punching is performed to prepare an aramid nonwoven fabric.
상기 중합용액, 다시말해 유기용매 내에 시아노기(-CN)가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액은 일정농도에서 액정성을 발현하기 때문에 이로 제조된 아라미드 공중합 필름은 고분자 사슬이 일축방향으로 배향된 구조를 갖는다.Since the polymerization solution, that is, the polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent, expresses liquid crystallinity at a certain concentration, the aramid copolymer film prepared therefrom is a polymer chain It has a uniaxially oriented structure.
그로인해, 일정 폭으로 슬리팅된 상기 아라미드 공중합 필름들을 적층한 후, 니들펀칭을 하게 되면 상기 아라미드 공중합 필름은 일축방향을 따라 섬유형태로 찢어지면서 피브릴을 형성하게되며, 그 결과 아라미드 부직포가 제조된다.Therefore, after laminating the aramid copolymer films slit to a certain width, and then needle punching, the aramid copolymer film is torn in the form of fibers along the uniaxial direction to form fibrils, and as a result, an aramid nonwoven fabric is manufactured do.
본 발명은 일정농도에서 액정성을 발현하는 공중합 아라미드 중합용액으로 제조되어 일축방향으로만 배향된 공중합 아라미드 필름을 사용하여 아라미드 부직포를 제조하기 때문에, 상기 니들펀칭공정에서 적층된 리본 형태의 공중합 아라미드 필름이 일측방향으로 쉽게 갈라지거나 찢어져 부직포를 형성할 수 있게 된다. 그로인해 본 발명은 종래 아라미드 부직포 제조를 위해 공중합 아라미드 중합용액을 섬유상으로 방사하는 공정을 생략할 수 있어서 제조공정이 간소화 된다.The present invention is prepared with a copolymer aramid polymerization solution that expresses liquid crystallinity at a certain concentration and uses a copolymer aramid film oriented only in uniaxial direction to prepare an aramid nonwoven fabric, so the copolymer aramid film in the form of a ribbon laminated in the needle punching process It is easily cracked or torn in one direction to form a nonwoven fabric. Therefore, the present invention can omit the process of spinning the copolymerized aramid polymerization solution into fibers for the production of the conventional aramid nonwoven fabric, thereby simplifying the manufacturing process.
이하, 실시예들을 통하여 본 발명을 보다 구체적으로 살펴본다. 그러나 본 발명의 보호범위를 하기 실시예만으로 한정해서 해석되어서는 안된다.Hereinafter, the present invention will be described in more detail through examples. However, it should not be construed as limiting the protection scope of the present invention only to the following examples.
실시예Example 1 One
3중량%의 염화칼슘(무기염)을 포함하는 N,N-디메틸아세트아미드(유기용매) 1,700g을 질소 분위기하에서 반응기에 넣고, 여기에 시아노-파라-페닐렌 디아민 110g을 투입하여 용해시켰다.1,700 g of N,N-dimethylacetamide (organic solvent) containing 3% by weight of calcium chloride (inorganic salt) was placed in a reactor under a nitrogen atmosphere, and 110 g of cyano-para-phenylene diamine was added thereto and dissolved.
이어서, 상기 반응기에 테레프탈로일 디클로라이드 250g을 첨가, 중합반응을 실시한 후 탄산리튬(중화제) 90g을 투입하여 중합용액을 제조하였다.Then, 250 g of terephthaloyl dichloride was added to the reactor to carry out a polymerization reaction, and then 90 g of lithium carbonate (neutralizing agent) was added to prepare a polymerization solution.
이어서, 200㎛ 갭(Gap)의 닥터블레이드를 사용하여 상기와 같이 제조된 중합용액을 유리판 위에 필름형태로 캐스팅한 후 50℃의 물에 침지하여 용매 및 금속염을 제거한 후, 200℃로 건조하여 공중합 아라미드 필름을 제조하였다.Then, using a doctor blade with a gap of 200 μm, the polymerization solution prepared as described above is cast in the form of a film on a glass plate, immersed in water at 50° C. to remove the solvent and metal salt, and then dried at 200° C. to copolymerize. An aramid film was prepared.
이어서, 제조된 공중합 아라미드 필름을 10㎜ 폭으로 슬리팅하여 리본 형태로 만든 다음, 웹(Web) 형태로 적층하고, 이를 니들펀칭하여 피브릴을 형성시켜 아라미드 부직포를 제조하였다. 제조된 아라미드 부직포를 육안으로 관찰 결과 리본 형태의 공중합 아라미드 필름이 니들펀칭에 의해 일측방향으로 섬유형태로 찢어지면서 피브릴이 잘 형성되어 있었다.Then, the prepared copolymer aramid film was slitted to a width of 10 mm to form a ribbon, then laminated in a web form, and needle punched to form fibrils to prepare an aramid nonwoven fabric. As a result of visual observation of the prepared aramid nonwoven fabric, fibrils were well formed as the ribbon-type copolymerized aramid film was torn into fibers in one direction by needle punching.
실시예Example 2 2
3중량%의 염화칼슘(무기염)을 포함하는 N,N-디메틸아세트아미드(유기용매) 1,700g을 질소 분위기하에서 반응기에 넣고, 여기에 시아노-파라-페닐렌 디아민 90g과 파라페닐렌디아민 40g을 투입하여 용해시켰다.1,700 g of N,N-dimethylacetamide (organic solvent) containing 3% by weight of calcium chloride (inorganic salt) was placed in a reactor under a nitrogen atmosphere, and 90 g of cyano-para-phenylene diamine and 40 g of para-phenylenediamine were placed there. was added and dissolved.
이어서, 상기 반응기에 테레프탈로일 디클로라이드 250g을 첨가, 중합반응을 실시한 후 산화칼슘(중화제) 95g을 투입하여 중합용액을 제조하였다.Then, 250 g of terephthaloyl dichloride was added to the reactor to carry out a polymerization reaction, and then 95 g of calcium oxide (neutralizing agent) was added to prepare a polymerization solution.
이어서, 200㎛ 갭(Gap)의 닥터블레이드를 사용하여 상기와 같이 제조된 중합용액을 유리판 위에 필름형태로 캐스팅한 후 50℃의 물에 침지하여 용매 및 금속염을 제거한 후, 200℃로 건조하여 공중합 아라미드 필름을 제조하였다.Then, using a doctor blade with a gap of 200 μm, the polymerization solution prepared as described above was cast in the form of a film on a glass plate, immersed in water at 50° C. to remove the solvent and metal salt, and then dried at 200° C. to copolymerize. An aramid film was prepared.
이어서, 제조된 공중합 아라미드 필름을 10㎜ 폭으로 슬리팅하여 리본 형태로 만든 다음, 웹(Web) 형태로 적층하고, 이를 니들펀칭하여 피브릴을 형성시켜 아라미드 부직포를 제조하였다. 제조된 아라미드 부직포를 육안으로 관찰 결과 리본 형태의 공중합 아라미드 필름이 니들펀칭에 의해 일측방향으로 섬유형태로 찢어지면서 피브릴이 잘 형성되어 있었다.Then, the prepared copolymer aramid film was slitted to a width of 10 mm to form a ribbon, then laminated in a web form, and needle punched to form fibrils to prepare an aramid nonwoven fabric. As a result of visual observation of the prepared aramid nonwoven fabric, fibrils were well formed as the ribbon-type copolymer aramid film was torn into fibers in one direction by needle punching.
Claims (4)
(ⅱ) 리본 형태로 슬리팅된 공중합 아라미드 필름을 적층한 후 니들펀칭하는 공정;을 포함하며,
상기 공중합 아라미드 필름은,
무기염이 첨가된 유기용매에 방향족 디아민 성분으로 파라페닐렌디아민과 시아노-파라-페닐렌 디아민을 1:9 ~ 9:1의 몰비로 용해시키거나 시아노-파라-페닐렌 디아민을 단독으로 용해시킨 다음, 상기 유기용매에 테레프탈로일 디클로라이드를 상기 방향족 디아민 성분의 총량과 동일한 몰량(Molar account)으로 첨가, 반응시켜 중합 반응을 실시한 후, 중화제를 투입하여 중합용액을 제조한 다음,
제조된 중합용액을 필름형태로 캐스팅하고, 캐스팅된 필름을 수세 및 건조하는 방법으로 제조되는 것을 특징으로 하는 공중합 아라미드 필름을 이용한 아라미드 부직포의 제조방법.(i) A copolymer aramid film having a thickness of 10 to 50 μm prepared by casting a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a cyano group (-CN) is dissolved in an organic solvent into a film shape is slit in a ribbon form ting (Slitting) process; and
(ii) a step of needle punching after laminating the copolymer aramid film slitted in the form of a ribbon;
The copolymer aramid film,
Paraphenylenediamine and cyano-para-phenylene diamine as an aromatic diamine component are dissolved in an organic solvent to which an inorganic salt is added in a molar ratio of 1:9 to 9:1, or cyano-para-phenylene diamine alone After dissolving, terephthaloyl dichloride is added to the organic solvent in the same molar amount as the total amount of the aromatic diamine component and reacted to conduct a polymerization reaction, and then a neutralizing agent is added to prepare a polymerization solution,
A method of manufacturing an aramid nonwoven fabric using a copolymerized aramid film, characterized in that it is prepared by casting the prepared polymerization solution in the form of a film, and washing and drying the cast film.
[상기 식(Ⅰ)에서 Ar은 하기 일반식(Ⅱ)의 방향족기고, 상기 A는 하기 일반식(Ⅲ)의 방향족기 이거나 하기 일반식(Ⅱ)의 방향족기와 일반식(Ⅲ)의 방향족기의 몰비가 1:9~9:1인 방향족기 이다]
[In the formula (I), Ar is an aromatic group of the following general formula (II), and A is an aromatic group of the following general formula (III) or an aromatic group of the following general formula (II) It is an aromatic group with a molar ratio of 1:9 to 9:1]
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